Adsorption chromatograph based method for recovering pleuromutilin from crystallization mother liquor

A technique of pleuromutilin and crystallization mother liquor, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry and other directions, can solve the problems of large impurity content, difficulty in separation and purification, waste of resources and the like, and achieves simple process, The effect of low production cost and improved industrial production efficiency

Inactive Publication Date: 2012-02-15
上海华震科技有限公司
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  • Summary
  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0006] In the pleuromutilin crystallization mother liquor, the content of pleuromutilin is 20-25%, and the rest are some solvents and most of the low-melting point oil-soluble impurities. The difficulty of separation and purification is relatively large, and the crystallization mother liquor is often treated as waste, which wastes resources, reduces the yield of pleuromutilin, increases production costs, and causes environmental pollution
There is no relevant literature report on the recovery and utilization of pleuromutilin in the mother liquor of pleuromutilin crystallization

Method used

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  • Adsorption chromatograph based method for recovering pleuromutilin from crystallization mother liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take 800 grams of pleuromutilin crystallization mother liquor vacuum concentrate and dissolve in 600g of methanol, stir evenly to make upper column liquid; then use a peristaltic pump to pump the upper column liquid into a 6L non-polar The upper part of the resin column of macroporous adsorption resin HZ816, and then use 18L of methanol aqueous solution eluent with a volume concentration of 66%, elute at a flow rate of 6L / h, collect and combine the eluent, concentrate in vacuo, evaporate the water, and recover the solvent , the concentrate was added with ethyl acetate to dissolve the crystals, and the crystals were vacuum-dried to obtain the finished product. The purity of the product obtained was determined by high performance liquid chromatography. In terms of mass fraction, the purity of pleuromutilin was 97.2%, and the total recovery rate was 90.1%.

Embodiment 2

[0024] Except that the non-polar macroporous adsorption resin HZ818 is used to replace the non-polar macroporous adsorption resin HZ816, other operations are the same as in Example 1. The measurement results, in terms of mass fraction, show that the purity of pleuromutilin is 95.7%, and the total recovery rate is 85.3%.

Embodiment 3

[0026] The chromatographic column was replaced with non-polar macroporous adsorption resin HZ830, and other operations were the same as in Example 1. As a result, the purity of pleuromutilin was 92.7% and the total recovery rate was 85.8% in terms of mass fraction.

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Abstract

An adsorption chromatograph based method for recovering pleuromutilin from a crystallization mother liquor, belongs to the technical field of separation and purification of antibiotic. The method is characterized by comprising steps of: carrying out a vacuum concentration on a pleuromutilin crystallization mother liquor, heating to 90 DEG C gradually until no distillate, adding water-soluble organic solvent and stirring uniformly; pumping into nonpolar macroporous adsorption resin column for adsorption; preparing an eluant by a water-soluble organic solvent with volume percentage of 20-70% and pumping into an adsorption resin column for desorption; carrying out vacuum condensation on the obtained eluate, adding organic solvent, dissolving, recrystallizing and carrying out vacuum drying to obtain a finished product. The invention has beneficial effects that the adsorption chromatograph based method for recovering pleuromutilin from the crystallization mother liquor has simple technique, low production costs, and a residual pleuromutilin recovery rate from the crystallization mother liquor reaches 85-92%, and a total production recovery rate reaches 95-98%, so as to increase industrial production efficiency.

Description

technical field [0001] The invention relates to a method for recovering pleuromutilin from pleuromutilin crystallization mother liquor by adsorption chromatography, and belongs to the technical field of separation and purification of antibiotics. Background technique [0002] Pleuromutilin can effectively inhibit most Gram-positive bacteria and some Gram-negative bacteria, Treponema (Helicobacter), Leptospirosis and Mycoplasma, etc. Pleuromutilin melting point: 170~172°C, dissolved in methanol, ethanol, chloroform and acetone. Pleuromutilin is a class of broad-spectrum diterpene antibiotics produced by Pleuromutilus, and its molecular structure is: [0003] [0004] The market application of pleuromutilin is mainly divided into three categories: first, it is mainly used for the production of derivatives such as tiamulin and warnimulin, accounting for about 89%; second, it is directly added to animal feed to prevent And treatment of infections caused by Gram, mycoplasma ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/675C07C67/56
Inventor 江邦和厉留柱徐环昕宁方红李大芦
Owner 上海华震科技有限公司
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